The increased interest in utilizing lignin as a feedstock
to produce
various aromatic compounds requires advanced chemical analysis methods
to provide qualitative and quantitative characterization of lignin
samples along different technology streamlines. However, due to the
lack of commercially available chemical standards, routine quantification
of industrially relevant lignin oligomers in complex lignin samples
remains a challenge. This study presents a novel method for universal
quantification of lignin dimers based on supercritical fluid chromatography
with charged aerosol detection (CAD). A series of lignin-derived dimeric
compounds that have been reported from reductive catalytic fractionation
(RCF) were synthesized and used as standards. The applicability of
using linear regression instead of quadratic calibration curves was
evaluated over a concentration range of 15–125 mg/L, demonstrating
that the former calibration method is as appropriate as the latter.
The response factors of lignin dimeric compounds were compared to
assess the uniformity of the CAD signal, revealing that the CAD response
for the tested lignin dimers did not differ substantially. It was
also found that the response factors were not dependent on the number
of methoxy groups or linkage motifs, ultimately enabling the use of
only one calibrant for these compounds. The importance of chromatographic
peak resolution in CAD was stressed, and the use of a digital peak
sharpening technique was adopted and applied to address this challenge.
The developed method was verified and used for the quantification
of lignin dimers in an oil obtained by a RCF of birch sawdust.